CN105895844A - Sticky ceramic diaphragm and preparation method thereof - Google Patents
Sticky ceramic diaphragm and preparation method thereof Download PDFInfo
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- CN105895844A CN105895844A CN201610233725.4A CN201610233725A CN105895844A CN 105895844 A CN105895844 A CN 105895844A CN 201610233725 A CN201610233725 A CN 201610233725A CN 105895844 A CN105895844 A CN 105895844A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/431—Inorganic material
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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Abstract
The invention discloses a preparation method of a sticky ceramic diaphragm. The method comprises the following steps: selecting a porous substrate; dipping the porous substrate into inorganic ceramic slurry and simultaneously stirring the inorganic ceramic slurry to evenly disperse the inorganic ceramic slurry on the surface of the porous substrate; drying the inorganic ceramic slurry to obtain a porous ceramic diaphragm; dipping the porous ceramic diaphragm into a glue solution and simultaneously stirring the glue solution to evenly disperse the glue solution on the surface of an inorganic ceramic coating of the porous ceramic diaphragm; and drying the glue solution to obtain the sticky ceramic diaphragm. The technology is simple. In a dipping manner, the double coated sticky ceramic diaphragm can be simultaneously formed, so that the problems of crimping, wrinkling and the like caused by secondary coating are solved; the thermal stability of the diaphragm is improved; and the yield of the product is improved. Meanwhile, an organic electrode adhesive coating is formed on the surface of a ceramic layer, so that achievement of efficiently automatic assembly is facilitated.
Description
Technical field
The present invention relates to technical field of lithium ion, be specifically related to a kind of viscous ceramic barrier film and preparation method thereof.
Background technology
In today that " energy-saving low-carbon " cry is the highest, development new-energy automobile is increasingly becoming the trend of contemporary automotive industry and is become, the research and development of all kinds of new energy technologies emerge in large numbers like the mushrooms after rain, lithium ion battery is as a kind of emerging " green energy-storing technology ", the most pollution-free, but also have that energy density is big, have extended cycle life, self discharge is little, memory-less effect, working range width, can the many merits such as fast charging and discharging, the most increasingly get more and more people's extensive concerning.
In lithium ion battery, electrokinetic cell has higher specific energy and specific power compared to communication class battery, therefore battery is under the conditions of short circuit, overcharging or cross and the non-normal use such as put, battery local temperature raises rapidly, when reaching the fusion temperature of barrier film, barrier film can occurrence of large-area shrink or fusing, causes both positive and negative polarity contact to cause internal short-circuit of battery, and then can cause the potential safety hazard such as battery catches fire or blast.The diaphragm material of lithium ion battery is usually polyolefin based materials at present, and its thermostability is poor, and wherein the closed pore temperature of polyethylene diagrams is 130～140 DEG C, and fusing-off temperature is at 150 DEG C, and polyacrylic temperature 150 DEG C of remaining silent, fusing-off temperature is at 170 DEG C.When battery temperature close to barrier film remain silent temperature time; the micropore of barrier film closes, and lithium ion can be stoped to continue transmission thus play the effect of liquid phase protection, but when temperature continuation rising reaches barrier film fusing-off temperature; barrier film fuses, and both positive and negative polarity will directly contact and produce internal short-circuit.Although now with safety three layers of composite diaphragm of higher polypropylene, polyethylene/polypropylene, but the electrokinetic cell requirement for barrier film safety can not be met, for the higher ternary system of specific energy, this is also that ternary material fails the key restriction factors of large-scale application.It addition, lithium ion battery is in long-term cyclic process, lithium metal deposit is easily formed Li dendrite, and traditional polyalkene diaphragm puncture strength is poor, and Li dendrite pierces through barrier film and both positive and negative polarity can be caused directly to contact, and causes internal short-circuit.In the face of these problems, improve the safety of dynamic lithium battery the most to a greater extent, it has also become focus of concern.
Up to the present, by having become as one of these problem most effective way of solution at membrane surface coated ceramic layer.The existence of inactive ceramic layer, can be obviously improved the puncture strength of barrier film, inorganic ceramic granule plays the effect of sept of a kind of physical form, can prevent the internal short-circuit caused because of diaphragm retracts, be obviously improved the security performance of lithium battery when battery is overheated.But at present the coating method of barrier film is all one side coating, and dual coating barrier film needs secondary to coat secondary baking, due to the most cated existence in secondary coating procedure, it is easily formed crimping, wrinkling, defective products rate are greatly promoted.
The additionally lithium battery of the structure type such as lamination or takeup type lamination, barrier film needs to adhere to each other with positive/negative plate in process, form stacking or the structure of folding, thus realizing efficient Automated assembly, the function how making ceramic diaphragm itself have adhesive electrodes pole piece is also the process needing constantly to explore, realize and continue to optimize.
Summary of the invention
Present invention seek to address that the problems referred to above, a kind of viscous ceramic barrier film and preparation method thereof is provided, the present invention solves secondary and coats the crimping caused, the problem such as wrinkling, improve the heat stability of barrier film, defective products rate is greatly promoted, the realization of the organic electrode adhesive layer of surface ceramii layer, is advantageously implemented Automated assembly efficiently simultaneously.
To achieve these goals, the invention provides the preparation method of a kind of viscous ceramic barrier film, comprise the following steps:
1) porous substrate is selected；
2) porous substrate be impregnated in inorganic ceramic slurry, and be stirred inorganic ceramic slurry making it be dispersed in the surface of porous substrate simultaneously；
3) it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；
4) porous ceramics barrier film be impregnated in glue, and be stirred glue making it be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film simultaneously；
5) it is dried, is formed with Double-plate machine high molecular bonding layer on the surface of porous ceramics barrier film, obtains viscous ceramic barrier film.
Further scheme, described porous substrate be porosity be the polyolefin-based substrates of 30-50%.
Scheme further, described inorganic ceramic slurry is made up of by mass percentage following components: inorganic ceramic granule 5%～40%, binding agent 2%～10%, dispersant 0.05%～2%, levelling agent 0.5%～3%, and remainder is solvent.
Further scheme, described inorganic ceramic granule be particle diameter be at least one in 100 nanometers～the aluminium oxide of 10 microns, boehmite, silicon oxide, titanium oxide, zirconium oxide, cerium oxide, magnesium oxide, nickel oxide, zinc oxide, barium sulfate, brium carbonate, silicon nitride, aluminium nitride, titanium nitride, boron nitride, Barium metatitanate., strontium titanates, carborundum.
Preferably, the particle diameter of described inorganic ceramic granule is 400～800 nanometers.
Scheme further, described binding agent is at least one in Kynoar, polyvinylidene fluoride-co-hexafluoropropene, butadiene-styrene rubber, polyvinyl alcohol, acrylonitrile multipolymer, polyacrylic acid, oleic series resin binder, acrylics binding agent；
Described dispersant is at least one in O-(2-aminopropyl)-O '-(2-methoxy ethyl) polypropylene glycol, Hypermer KD-1, Hypermer KD-3, polyvinylpyrrolidone, sub-sodium silicate, tetramethyl ammonium hydroxide, polyacrylic acid, POLYPROPYLENE GLYCOL, polypropylene, Fructus Citri Limoniae acid amide, Polyethylene Glycol, sodium polyacrylate；Wherein Hypermer
KD-1、Hypermer
KD-3 is Britain's standing grain big conducting powder dispersant special.
Described levelling agent is at least one in silicone, acrylic compounds, fluorine carbon；Wherein silicone is modified polyorganosiloxane, polyether-modified polydimethylsiloxane etc..
Described solvent is N-Methyl pyrrolidone, N-N-dimethylformamide, acetone, isopropanol or deionized water.
Scheme further, described glue is at least one in polymethyl methacrylate, acrylate based polyalcohol, sodium carboxymethyl cellulose, Kynoar, polyvinylidene fluoride-co-hexafluoropropene, butadiene-styrene rubber, polypropylene acid or acrylonitrile multiple aggregation composition glue liquid；The solid content of described glue is 0.5%-10%.
Further scheme, described step 3), 5) in baking temperature be 20-70oC。
Further scheme, described step 2), 4) in mixing speed less than 300 rpm.
Another goal of the invention of the present invention is to provide a kind of viscous ceramic barrier film prepared through above-mentioned preparation method.
In the present invention, the porosity of polyolefin-based substrates is 30%-50%, preferably 40%-45%；The thickness of polyolefin-based substrates is 1-40 micron, preferably 9-32 micron；
The inorganic ceramic granule that the present invention selects be particle diameter be 100 nanometers～10 microns, owing to its particle diameter is the least, it is difficult to dispersion, easily reunite during scattered, therefore need to use dispersant in inorganic ceramic slurry, and need incessantly it to be carried out high speed dispersion in dipping process, so that it is evenly dispersed in the surface of porous substrate.
Porous substrate impregnated in formation double-surface ceramics layer in inorganic ceramic slurry, and ceramic particle on porous substrate surface and is adhered to each other by adhesive bond, the gap between granule constitutes hole；Make solvent evaporate through being dried, form porous ceramics barrier film.Again through the second dipping of glue, concurrently form two-sided organic polymer adhesive layer at surface ceramii layer, after solvent is dried, form organic high molecular bonding layer on ceramic diaphragm surface.
I.e. the present invention is by the way of dipping, first concurrently form inorganic, ceramic layer on the two sides of porous substrate, again by dipping glue after drying, and concurrently form organic adhesive layer at barrier film surface ceramii layer, double-surface ceramics layer and two-sided organic layer concurrently form respectively, thus solve secondary and coat the crimping caused, the problem such as wrinkling, and improve the heat stability of barrier film, improve the yields of product；It is formed with machine electrode adhesive layer at surface ceramii layer simultaneously, is advantageously implemented Automated assembly efficiently.
It addition, the present invention can control inorganic, ceramic layer and the thickness of organic polymer adhesive layer by the concentration controlling inorganic ceramic slurry and glue.
Accompanying drawing explanation
The present invention is further detailed explanation with detailed description of the invention below in conjunction with the accompanying drawings.
Fig. 1 is the porous ceramics barrier film SEM figure of embodiment 1 preparation；
Fig. 2 is the viscous ceramic barrier film SEM figure of embodiment 1 preparation.
Detailed description of the invention
Embodiment 1
1) PP selecting 25 microns of thickness, porosity to be 45% is porous substrate；
By inorganic ceramic particulate alumina (Al2O3) 13%, binding agent acrylonitrile multipolymer (LA133) 5%, polyethylene of dispersing agent ketopyrrolidine 1.5%, levelling agent modified polyorganosiloxane 0.5%, remainder is solvent deionized water, carries out high speed dispersion and is allowed to form homogeneous inorganic ceramic slurry；
Select polymethyl methacrylate and acetone to be fully stirred dissolving by weight 3:97 and make glue.
2) porous substrate be impregnated in inorganic ceramic slurry, and inorganic ceramic slurry is stirred with mixing speed 30 rpm simultaneously so that it is be dispersed in the surface of porous substrate；
3) with 55 DEG C, it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；4) porous ceramics barrier film be impregnated in glue, and glue is stirred with mixing speed 30 rpm simultaneously so that it is be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film；
5) with 50 DEG C, it is dried, is formed with Double-plate machine high molecular bonding layer on the surface of porous ceramics barrier film, obtains viscous ceramic barrier film.
It is illustrated in figure 1 the SEM figure of porous ceramics barrier film, as can be seen from Figure 1, defines homogeneous ceramic coating on the surface of porous substrate；
It is the SEM figure of viscous ceramic barrier film as shown in Figure 2, as can be seen from Figure 2, at one layer of organic polymer layer of surface uniform fold of ceramic coating, then proves to define the viscous ceramic barrier film of Organic-inorganic composite.
Embodiment 2
1) PE selecting 20 microns of thickness, porosity to be 50% is porous substrate；
By inorganic ceramic granule boehmite (AlO (OH)) 40%, binding agent polyacrylic acid 10%, dispersant Asia sodium silicate 0.05%, the polyether-modified polydimethylsiloxane of levelling agent 0.5%, remainder is solvent N-methyl pyrilidone, carries out high speed dispersion and is allowed to form homogeneous inorganic ceramic slurry；
Select polyvinylidene fluoride-co-hexafluoropropene, N-Methyl pyrrolidone and make glue by weight 2.5:97.5 stirring and dissolving.
2) porous substrate be impregnated in inorganic ceramic slurry, and inorganic ceramic slurry is stirred with mixing speed 100 rpm simultaneously so that it is be dispersed in the surface of porous substrate；
3) with 30 DEG C, it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；
4) porous ceramics barrier film be impregnated in glue, and glue is stirred with mixing speed 100 rpm simultaneously so that it is be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film；
5) with 20 DEG C, it is dried, is formed with Double-plate machine high molecular bonding layer on the surface of porous ceramics barrier film, obtains viscous ceramic barrier film.
Embodiment 3
1) PP selecting 25 microns of thickness, porosity to be 30% is porous substrate；
By inorganic ceramic granule barium sulfate (BaSO4) 5%, binding agent Kynoar 2%, dispersant Hypermer KD-1 2%, levelling agent modified polyorganosiloxane 3%, remainder is solvent isopropanol, is sufficiently mixed, and carries out high speed dispersion and be allowed to form homogeneous inorganic ceramic slurry；
Sodium carboxymethyl cellulose and acetone is selected to be sufficiently stirred for making glue by weight 10:90.
2) porous substrate be impregnated in inorganic ceramic slurry, and inorganic ceramic slurry is stirred less than 50 rpm with mixing speed simultaneously so that it is be dispersed in the surface of porous substrate；
3) with 70 DEG C, it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；
4) porous ceramics barrier film be impregnated in glue, and glue is stirred less than 50 rpm with mixing speed simultaneously so that it is be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film；
5) with 70 DEG C, it is dried, is formed with Double-plate machine high molecular bonding layer on the surface of porous ceramics barrier film, obtains viscous ceramic barrier film.
Embodiment 4
1) PP selecting 25 microns of thickness, porosity to be 40% is porous substrate；
By the carborundum 20% that particle diameter is 100 nanometers, binding agent polyvinyl alcohol 10%, dispersant Polyethylene Glycol 0.1%, levelling agent acrylic compounds 0.5%～3%, remainder is solvent N-N-dimethylformamide, is sufficiently mixed, and carries out high speed dispersion and be allowed to form homogeneous inorganic ceramic slurry；
Butadiene-styrene rubber and acetone is selected to make glue for 0.5:95.5 stirring in mass ratio.
2) porous substrate be impregnated in inorganic ceramic slurry, and inorganic ceramic slurry is stirred less than 200 rpm with mixing speed simultaneously so that it is be dispersed in the surface of porous substrate；
3) with 30 DEG C, it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；
4) porous ceramics barrier film be impregnated in glue, and glue is stirred less than 200 rpm with mixing speed simultaneously so that it is be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film；
5) with 20 DEG C, it is dried, is formed with Double-plate machine high molecular bonding layer on the surface of porous ceramics barrier film, obtains viscous ceramic barrier film.
Above content is only the structure example to the present invention and explanation; described specific embodiment is made various amendment or supplements or use similar mode to substitute by affiliated those skilled in the art; without departing from the structure of the present invention or surmount scope defined in the claims, protection scope of the present invention all should be belonged to.
Claims (10)
1. the preparation method of a viscous ceramic barrier film, it is characterised in that: its preparation process includes:
1) porous substrate is selected；
2) porous substrate be impregnated in inorganic ceramic slurry, and be stirred inorganic ceramic slurry making it be dispersed in the surface of porous substrate simultaneously；
3) it is dried, forms two-sided inorganic ceramic coating on the surface of porous substrate, obtain porous ceramics barrier film；
4) porous ceramics barrier film be impregnated in glue, and be stirred glue making it be dispersed in the surface of the inorganic ceramic coating of porous ceramics barrier film simultaneously；
5) it is dried, forms two-sided organic polymer adhesive layer on the surface of porous ceramics barrier film, obtain viscous ceramic barrier film.
Preparation method the most according to claim 1, it is characterised in that: described porous substrate be porosity be the polyolefin-based substrates of 30-50%.
Preparation method the most according to claim 1, it is characterized in that: described inorganic ceramic slurry is made up of by mass percentage following components: inorganic ceramic granule 5%～40%, binding agent 2%～10%, dispersant 0.05%～2%, levelling agent 0.5%～3%, remainder is solvent.
Preparation method the most according to claim 3, it is characterised in that: described inorganic ceramic granule be particle diameter be at least one in 100 nanometers～the aluminium oxide of 10 microns, boehmite, silicon oxide, titanium oxide, zirconium oxide, cerium oxide, magnesium oxide, nickel oxide, zinc oxide, barium sulfate, brium carbonate, silicon nitride, aluminium nitride, titanium nitride, boron nitride, Barium metatitanate., strontium titanates, carborundum.
Preparation method the most according to claim 4, it is characterised in that: the particle diameter of described inorganic ceramic granule is 100 nanometers～10 microns.
Preparation method the most according to claim 3, it is characterised in that: described binding agent is at least one in Kynoar, polyvinylidene fluoride-co-hexafluoropropene, butadiene-styrene rubber, polyvinyl alcohol, acrylonitrile multipolymer, polyacrylic acid, oleic series resin binder, acrylics binding agent；
Described dispersant is O-(2-aminopropyl)-O '-(2-methoxy ethyl) polypropylene glycol, Hypermer KD-1, Hypermer
At least one in KD-3, polyvinylpyrrolidone, sub-sodium silicate, tetramethyl ammonium hydroxide, polyacrylic acid, POLYPROPYLENE GLYCOL, polypropylene, Fructus Citri Limoniae acid amide, Polyethylene Glycol, sodium polyacrylate；
Described levelling agent is at least one in silicone, acrylic compounds, fluorine carbon；
Described solvent is N-Methyl pyrrolidone, N-N-dimethylformamide, acetone, isopropanol or deionized water.
Preparation method the most according to claim 1, it is characterised in that: described glue is at least one in polymethyl methacrylate, acrylate based polyalcohol, sodium carboxymethyl cellulose, Kynoar, polyvinylidene fluoride-co-hexafluoropropene, butadiene-styrene rubber, polypropylene acid or acrylonitrile multiple aggregation composition glue liquid；The solid content of described glue is 0.5%-10%.
Preparation method the most according to claim 1, it is characterised in that: described step 3), 5) in baking temperature be 20-70 DEG C.
Preparation method the most according to claim 1, it is characterised in that: described step 2), 4) in mixing speed less than 300 rpm.
10. the viscous ceramic barrier film that prepared by a preparation method as claimed in claim 1.
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| CN106549128A (en) * | 2017-01-19 | 2017-03-29 | 宁德卓高新材料科技有限公司 | A kind of non-all standing formula coats the preparation method of barrier film |
| CN106784533A (en) * | 2017-01-20 | 2017-05-31 | 东莞市卓高电子科技有限公司 | A kind of production technology containing PMMA and its copolymer coated barrier film |
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